Efficient and energy-saving building thermal insulation material and preparation method thereof
By employing a multi-component synergistic design and gradient mixing process involving modified aerogels, composite mineral fibers, and phase change energy storage microcapsules, the problem of insufficient performance synergy in existing building thermal insulation materials has been solved, thereby improving the structural stability and thermal insulation performance of the materials.
Patent Information
- Application Number
- CN202511844476.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-09
- Publication Date
- 2026-02-27
AI Technical Summary
Existing building insulation materials are insufficient in terms of overall performance synergy, making it difficult to achieve a balanced approach to insulation, reinforcement, and structural stability.
The method employs a multi-component synergistic formulation of modified aerogel, composite mineral fiber, and phase change energy storage microcapsules. The modification process enhances the compatibility and interfacial bonding between the components, while a gradient mixing process ensures uniform dispersion and synergistic effect of each component.
It achieves a balanced improvement in the overall performance of building thermal insulation materials, ensuring structural stability and thermal insulation performance, and the materials have self-healing capabilities during thermal aging.
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Figure CN121573928A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application relates to the technical field of building materials, in particular to a high-efficiency energy-saving building thermal insulation material and a preparation method thereof. BACKGROUND
[0002] Building energy saving is one of the core directions of the current building industry, and building thermal insulation materials, as key components for reducing building energy consumption, directly affect the energy-saving effect and use safety of buildings. An ideal building thermal insulation material should have excellent thermal insulation performance, reliable mechanical strength and stable structural properties to meet the comprehensive needs of thermal insulation, load bearing and support and aging resistance during long-term use, and plays a key role in the application of building outer walls, roofs and other parts.
[0003] However, the existing building thermal insulation materials generally have insufficient performance synergy, and it is difficult to balance the core performances such as thermal insulation, reinforcement and structural stability. Some materials rely on a single thermal insulation component to achieve thermal insulation effect, but the mechanical strength is weak and easy to break during installation or use; some materials focus on improving mechanical properties, but sacrifice the thermal insulation efficiency, with a high thermal conductivity coefficient; some materials try to composite multiple components, but due to the lack of scientific proportioning design, targeted modification of key raw materials, or poor functional synergy between components, the overall structural stability of the material is insufficient, and the performance decays significantly after long-term use, which cannot meet the stringent requirements of buildings on the comprehensive performance of thermal insulation materials.
[0004] The patent with publication number CN108675685A discloses a kind of high-efficiency energy-saving building thermal insulation material and its preparation method, which uses building wood waste, ceramic waste and other industrial waste as main raw materials, and is compounded with silicon dioxide aerogel, modified polystyrene and other components to realize basic thermal insulation and mechanical properties through simple modification. However, the thermal insulation mechanism of this scheme is relatively simple, relying only on the low thermal conductivity of aerogel and the porous structure of foamed polystyrene, without forming a multi-component synergistic insulation system, and lacking precise modification and functional adaptation design of key components. Each component only has a single function, and cannot achieve the synergistic balance of thermal insulation, reinforcement and structural stability. At the same time, the preparation process lacks fine component pretreatment and mixing control, making it difficult to ensure the uniformity and long-term stability of material performance, and failing to solve the core problem of the imbalance of the comprehensive performance of existing materials. The present application solves the problem of insufficient performance synergy in existing technology and the comparative document by modifying aerogel, compounding mineral fibers and phase change energy storage microcapsules, and performing targeted modification of key raw materials. The mineral fibers are composed of basalt fibers and ceramic fibers in a specific ratio, so that each component can play the roles of thermal insulation, reinforcement and energy storage and form a synergistic effect, thus achieving balanced improvement of the comprehensive performance of the material. SUMMARY
[0005] In order to solve the problem of insufficient comprehensive performance synergy of building thermal insulation materials in the prior art, the application provides a high-efficiency and energy-saving building thermal insulation material and a preparation method.
[0006] In a first aspect, the application provides a high-efficiency and energy-saving building thermal insulation material, which adopts the following technical scheme: A high-efficiency and energy-saving building thermal insulation material is made of the following components by weight: 15-25 parts of modified aerogel, 20-30 parts of composite mineral fiber, 8-15 parts of phase change energy storage microcapsule, 5-10 parts of nano silicon dioxide, 10-18 parts of water-based epoxy resin, 3-8 parts of polyamide curing agent, 12-20 parts of expanded perlite, 6-12 parts of hollow glass microbeads, 2-5 parts of hydroxypropyl methyl cellulose, 3-7 parts of amino-modified polyurethane microspheres, and 2-6 parts of nano boron nitride.
[0007] By adopting the above technical scheme, a multi-dimensional thermal insulation system is formed by the modified aerogel and the nano boron nitride, which plays a role in blocking heat transfer; a support framework is built by the basalt fiber and the ceramic fiber in the composite mineral fiber, which plays a role in enhancing the structural strength of the material; the interstitial gaps between components are filled by the amino-modified polyurethane microspheres, which plays a role in optimizing the interface bonding; the adsorption and release of heat are adjusted by the phase change energy storage microcapsule, which plays a role in buffering temperature fluctuations; a bonding matrix is formed by the water-based epoxy resin and the polyamide curing agent, which plays a role in firmly combining the components; the porous structure is introduced by the expanded perlite and the hollow glass microbeads, which plays a role in reducing the density of the material and assisting in thermal insulation; the dispersibility and formability of the system are improved by the nano silicon dioxide and the hydroxypropyl methyl cellulose, which plays a role in improving the uniformity of the material structure, thereby achieving the effect of complementary functions of the components and collaborative construction of high-performance thermal insulation materials.
[0008] Preferably, the modified aerogel is silica aerogel modified by surface grafting with a silane coupling agent; the particle size of the amino-modified polyurethane microspheres is 1-5 pm, and the surface amino content is 0.8-1.5 mmol / g.
[0009] By adopting the above technical scheme, the silica aerogel is surface grafted and modified by the silane coupling agent, which plays a role in optimizing the surface activity of the aerogel and improving the interface bonding force between the aerogel and the bonding system and other functional components; the specific particle size range and surface amino content of the amino-modified polyurethane microspheres are limited, which plays a role in making the microspheres more easily fill the interstitial gaps between the components and form stable interactions with other components through the surface amino groups, thereby achieving the effect of precise function of the two modified raw materials in the material system and collaborative adaptation with other components, effectively guaranteeing the structural stability and thermal insulation performance of the material.
[0010] Preferably, the core material of the phase change energy storage microcapsule is polyethylene glycol 6000, and the wall material is melamine formaldehyde resin, the particle size of the phase change energy storage microcapsule is 5-20 μm; the lamellar thickness of the nano boron nitride is 5-20 nm, and the lateral size is 0.5-2 μm.
[0011] By adopting the above technical scheme, by selecting polyethylene glycol 6000 as the core material of the phase change energy storage microcapsule, using its phase change characteristics suitable for building thermal insulation scene to play the role of efficient absorption and release of heat, using melamine formaldehyde resin as the wall material to play the role of stable wrapping the core material and preventing the leakage of phase change material, limiting the microcapsule particle size to 5-20 μm to play the role of ensuring its uniform dispersion in the material system and full contact to play the energy storage function; by limiting the lamellar thickness of the nano boron nitride to 5-20 nm and the lateral size to 0.5-2 μm, the lamellar structure of the nano boron nitride is fully spread to form a heat blocking network, and the size is adapted to other components for easy dispersion, thereby achieving the role of synergistic adaptation of phase change energy storage and physical heat insulation function, stable play, and ensuring the persistence and reliability of the material thermal insulation performance.
[0012] Preferably, the composite mineral fiber comprises basalt fiber and ceramic fiber, and the mass ratio of basalt fiber to ceramic fiber is 3:1-2:1.
[0013] By adopting the above technical scheme, by selecting basalt fiber and ceramic fiber to form a composite mineral fiber, by virtue of the high strength characteristics of basalt fiber to play the role of supporting the material structure and improving the mechanical properties, by virtue of the excellent heat insulation and high temperature resistance characteristics of ceramic fiber to play the role of assisting heat transfer, and by limiting the mass ratio of the two to 3:1-2:1, the performance advantages of the two fibers are precisely matched, and the shortcomings of single fiber characteristics are avoided, thereby achieving the role of the composite mineral fiber which can provide stable structural support for the material and synergistically play a role with other heat insulation components, and ensuring the balanced adaptation of the mechanical properties and thermal insulation performance of the material.
[0014] In a second aspect, the application provides a preparation method of a high-efficiency energy-saving building thermal insulation material, which adopts the following technical scheme: A preparation method of a high-efficiency energy-saving building thermal insulation material, comprising the following steps: S1, composite mineral fiber pretreatment: after high temperature activation treatment of the composite mineral fiber, the composite mineral fiber is immersed in a silane coupling agent solution and dried to obtain modified composite mineral fiber; S2, amino-modified polyurethane microsphere activation: the amino-modified polyurethane microspheres are subjected to plasma treatment to obtain activated polyurethane microspheres; S3, multi-component synergistic dispersion: dispersing the phase change energy storage microcapsules, nano boron nitride and the activated polyurethane microspheres obtained in step S2 in a liquid medium containing a dispersing agent by stirring and ultrasonic treatment to obtain a multi-component suspension; S4, adhesive system preparation: mixing the water-based epoxy resin and the polyamide curing agent, then adding hydroxypropyl methyl cellulose and nano silicon dioxide, and continuously stirring to form an adhesive system; S5, gradient mixture preparation: first, mixing the modified composite mineral fibers obtained in step S1 with expanded perlite, hollow glass microbeads and modified aerogel by primary stirring; then, adding the multi-component suspension prepared in step S3 for secondary stirring; finally, adding the adhesive system prepared in step S4 for tertiary stirring, and mixing uniformly under the protection of inert gas; S6, molding and post-processing: injecting the mixture obtained in step S5 into a preheated mold for compression molding and demolding; heat treating the molded body after demolding; and finally, curing under controlled temperature and humidity conditions to obtain the building thermal insulation material.
[0015] By adopting the above technical scheme, the composite mineral fibers are subjected to high-temperature activation and silane coupling agent impregnation drying in step S1, which plays a role in removing impurities on the fiber surface, improving surface activity and compatibility with subsequent components; the amino-modified polyurethane microspheres are subjected to plasma treatment in step S2, which plays a role in further activating the functional groups on the surface of the microspheres and strengthening their interaction with other components; the multi-component is dispersed in a liquid medium by stirring and ultrasonic combination in step S3, which plays a role in breaking agglomeration and achieving uniform distribution of small components; the adhesive system is prepared step by step in step S4, which plays a role in ensuring that the related components of the adhesive are fully integrated to form a stable adhesive matrix; the gradient tertiary stirring is adopted in step S5 and assisted by inert gas protection, which plays a role in adapting to the characteristics of different components and avoiding secondary agglomeration or oxidation of the components during the mixing process; the material is shaped and densified, and the structure is stably solidified in step S6 by preheating the mold, heat treatment and curing under specified temperature and humidity conditions, which plays a role in achieving the effect of fully exerting the functions of each component through layer-by-layer connection and synergistic guarantee in each preparation link, and finally obtaining a thermal insulation material with uniform structure and stable performance.
[0016] Preferably, in step S1, the temperature of the high-temperature activation treatment is 500-600℃, and the time is 2-3h; the mass concentration of the silane coupling agent solution is 1-3%, and the impregnation time is 30-60min; the drying temperature is 100-120℃, and the time is 1-2h; and the silane coupling agent is γ-aminopropyl triethoxysilane; in step S2, the plasma treatment is carried out in an argon atmosphere, the treatment frequency is 13.56MHz, the treatment power is 80-120W, the treatment chamber pressure is 10-20Pa, and the treatment time is 5-10min.
[0017] By adopting the technical scheme, the temperature and time of high-temperature activation treatment are limited in step S1, which plays a role of fully removing the surface impurities of the composite mineral fiber and activating the surface active sites of the fiber. The γ-aminopropyl triethoxysilane is selected and the mass concentration of the solution and the impregnation time are limited, which plays a role of allowing the coupling agent molecules to be fully grafted to the fiber surface and precisely regulating the modification degree. The temperature and time of drying are limited, which plays a role of removing the excess water on the fiber surface, stabilizing the grafting effect and not damaging the fiber structure. The plasma treatment is performed in an argon atmosphere in step S2, which plays a role of avoiding the oxidation of the microsphere surface. The treatment frequency, power, chamber pressure and time are limited, which plays a role of precisely activating the surface functional groups of the amino-modified polyurethane microspheres, improving the reactivity and not damaging the properties of the microspheres. Thus, the modification effect of the composite mineral fiber and the amino-modified polyurethane microspheres is controllable, which lays a good foundation for the subsequent combination of various components.
[0018] Preferably, in step S3, the stirring speed is 3000-5000 r / min and the time is 20-30 min. The ultrasonic treatment power is 200-300 W and the time is 15-25 min. After the activated polyurethane microspheres are added, ultrasonic treatment is continued for 5-10 min. The dispersing agent is a compound of polyethylene glycol octylphenyl ether and sodium dodecyl sulfate in a mass ratio of 2:1, and the addition amount is 0.5-1.5% of the total mass of the phase change energy storage microcapsules and nano boron nitride.
[0019] By adopting the technical scheme, the stirring speed of 3000-5000 r / min and the stirring time of 20-30 min in step S3 are limited, which plays a role of quickly dispersing the initial agglomerates of the phase change energy storage microcapsules and nano boron nitride. The ultrasonic power of 200-300 W and the ultrasonic time of 15-25 min are set, which plays a role of breaking the fine agglomeration and refining the dispersed particles. After the activated polyurethane microspheres are added, ultrasonic treatment is continued for 5-10 min, which plays a role of allowing the microspheres to fully contact with other dispersed components and avoiding local aggregation. The dispersing agent is a compound of polyethylene glycol octylphenyl ether and sodium dodecyl sulfate in a mass ratio of 2:1, which plays a role of improving the dispersion stability of the system by means of the synergistic dispersion effect of the two components. The addition amount is limited to 0.5-1.5% of the total mass of the phase change energy storage microcapsules and nano boron nitride, which plays a role of precisely regulating the dispersion effect and avoiding the excessive dispersing agent from affecting other properties of the material. Thus, the multiple components are uniformly and stably dispersed in the liquid medium, which lays a foundation for the subsequent gradient mixing and balanced overall performance of the material.
[0020] Preferably, in step S4, the temperature of the mixing is 40-50℃; the stirring speed when adding the polyamide curing agent is 500-800r / min, and the mixing time is 10-15min; the stirring time after adding the hydroxypropyl methyl cellulose and nano-silica is 20-30min.
[0021] By adopting the above technical solution, by limiting the mixing temperature of 40-50℃ in step S4, the reaction activity of the water-based epoxy resin and the polyamide curing agent is adapted, the uniform fusion of the two is promoted, and the inherent characteristics of the components are not damaged; by setting the stirring speed of 500-800r / min and the mixing time of 10-15min when adding the polyamide curing agent, the curing agent is quickly and uniformly dispersed in the epoxy resin, and the local curing reaction imbalance is avoided; by extending the stirring time to 20-30min after adding the hydroxypropyl methyl cellulose and nano-silica, the thickening components are fully dissolved, the nano-silica is broken and uniformly embedded in the bonding matrix, thereby achieving the effect of fully fused components, stable structure and good adaptability of the bonding system, which provides protection for subsequent firm combination with other functional components.
[0022] Preferably, in step S5, the rotation speed of the first-stage stirring is 200-300r / min, and the time is 10-15min; the rotation speed of the second-stage stirring is 800-1000r / min, and the time is 20-30min; the rotation speed of the third-stage stirring is 1500-2000r / min, and the time is 30-40min; the inert gas is nitrogen or argon, and the gas inlet rate is 0.5-1L / min.
[0023] By adopting the above technical solution, by limiting the low rotation speed of 200-300r / min and the time of 10-15min of the first-stage stirring in step S5, for the relatively coarse particle components such as modified composite mineral fibers and expanded perlite, the effect of gentle mixing, avoiding component crushing and achieving preliminary uniform distribution is achieved; by increasing the rotation speed of the second-stage stirring to 800-1000r / min and extending the time to 20-30min, the fine dispersion characteristics of the multi-component suspension are adapted, the effect of fully wetting contact between the fine components and the coarse particles is achieved, and the stratified agglomeration is avoided; by further increasing the rotation speed to 1500-2000r / min and extending the time to 30-40min in the third-stage stirring, the effect of thoroughly fusing all components and uniformly wrapping the functional components by the bonding matrix is achieved after adding the bonding system; nitrogen or argon is selected as the inert gas, and the inlet rate is limited to 0.5-1L / min, the effect of isolating air, preventing oxidation of components during mixing and maintaining system stability is achieved, thereby achieving the effects of gradient adaptation of mixing intensity and time according to component characteristics, close fusion of components and uniform distribution, and ensuring the consistency of the overall performance of the material.
[0024] Preferably, in step S6, the preheating temperature of the mold is 60-80℃, the pressing pressure is 5-8MPa, and the pressure holding time is 15-20min; the heat treatment is carried out at 150-200℃ for 2-3h, the heating rate is 5-10℃ / min, and the mold is naturally cooled to room temperature after heat treatment; the curing environment temperature is 25-30℃, the relative humidity is 60-70%, and the curing time is 7-10 days.
[0025] By adopting the above technical scheme, by limiting the preheating temperature of the mold in step S6 to be 60-80℃, the mixture is uniformly heated when contacting the mold, and internal stress or forming defects caused by temperature difference are avoided; by setting the pressing pressure to be 5-8MPa and the pressure holding time to be 15-20min, the material is fully densified, the components are closely attached, and the forming size is stable; by controlling the heat treatment temperature to be 150-200℃, the heat treatment time to be 2-3h, and the heating rate to be 5-10℃ / min, the bonding system is completely solidified, the bonding force between the components is strengthened, and material cracking caused by sudden temperature rise is avoided, and the internal residual stress is further reduced after natural cooling after heat treatment; by limiting the curing environment temperature to be 25-30℃, the relative humidity to be 60-70%, and the curing time to be 7-10 days, the material continuously and stably reacts under mild conditions, and the structural integrity is improved, thereby achieving the effects of excellent forming quality, dense and stable material structure, and fully developed performance, and ensuring the use reliability of the final product.
[0026] In summary, the present application has the following beneficial effects: 1. The present application adopts a multi-component synergistic matching of modified aerogel, composite mineral fiber, phase change energy storage microcapsule, etc., the dosages of each component are reasonably limited, the composite mineral fiber is combined with basalt fiber and ceramic fiber in a specific ratio, the key raw materials such as modified aerogel are subjected to targeted modification treatment, and each component plays the roles of heat insulation, reinforcement, energy storage, etc. in the material system, and cooperatively forms a composite system with stable structure, thereby achieving the effect of balanced comprehensive performance.
[0027] 2. In the present application, silica aerogel modified by surface grafting of silane coupling agent, amino-modified polyurethane microspheres with specific particle size and amino content, and phase change energy storage microcapsules and nano boron nitride with specific structure parameters are preferably used. The properties of these preferred raw materials are more suitable for other components, which can reduce interface defects and strengthen the interaction between components, thereby achieving the effect of more stable material function.
[0028] 3、The method of the application, through composite mineral fiber pretreatment, amino modified polyurethane microsphere plasma activation, multi-component synergistic dispersion and gradient mixing and other steps, combined with precise control of various process parameters, ensures the uniform dispersion of various components in the material, promotes the interface bonding between the components, and improves the material structure density through heat treatment and standard curing, so as to obtain the effect of more optimal material performance stability.
[0029] 4、The application forms a good interface combination with other components through its own characteristics, which helps to improve the bearing capacity of the material and plays a certain self-repairing or structural reinforcing role in the heat aging process.
[0030] 5、The application improves the compatibility of aerogel and other components through modification of aerogel, reduces interface defects, makes it more difficult to form heat transfer path, and also enhances the bonding strength of aerogel and matrix. BRIEF DESCRIPTION OF DRAWINGS
[0031] Figure 1 is a preparation method flow chart of a high-efficiency energy-saving building thermal insulation material provided by the application. DETAILED DESCRIPTION
[0032] The application will be further described in detail below in combination with examples and comparative examples, wherein the experimental methods used below are conventional methods unless otherwise specified. The materials, reagents, methods and instruments used are conventional materials, reagents, methods and instruments in the art unless otherwise specified, and can be obtained or prepared according to the literature method by those skilled in the art.
[0033] Technical idea: The existing building thermal insulation materials have the problem of insufficient comprehensive performance synergy, and the core reason is that the related technology lacks scientific multi-component synergistic design and precise performance adaptation mechanism: some schemes rely on single functional components, resulting in mutual restriction of thermal insulation, mechanical strength, structural stability and other performances; although some composite schemes are equipped with multiple components, the key raw materials are not modified, and the component ratio lacks optimization, resulting in weak interface bonding between components and poor functional synergy effect; at the same time, the preparation process mostly adopts simple mixing mode, without fine control according to the component characteristics, further exacerbating the problem of uneven performance.
[0034] The technical scheme solves the above problems through the combination of component synergistic design, precise modification and fine process: firstly, functional complementary components such as modified aerogel, composite mineral fiber and phase change energy storage microcapsule are screened, the amount of each component is reasonably limited, and the composite mineral fiber is combined with basalt fiber and ceramic fiber in a specific ratio, so that each component bears the functions of heat insulation, reinforcement and energy storage respectively; secondly, the key raw materials such as modified aerogel and composite mineral fiber are modified and treated, so as to improve the compatibility and interface bonding force between the components; finally, the fine preparation process such as composite mineral fiber pretreatment, plasma activation of amino-modified polyurethane microspheres, multi-component synergistic dispersion and gradient mixing is designed, so as to ensure the uniform dispersion and full synergy of each component, and finally a stable composite system is constructed, and the comprehensive performance of the material is balancedly improved.
[0035] Preparation Example 1 The preparation method of the modified aerogel is as follows: 100 parts of silica aerogel powder was dispersed in 500 parts of anhydrous ethanol, stirred at a speed of 300 r / min for 30 min to form a uniform suspension; a silane coupling agent γ-aminopropyl triethoxysilane was taken in a proportion of 3-5% of the mass of the silica aerogel, dissolved in 100 parts of a mixed solvent of ethanol and deionized water in a volume ratio of 3:1, and stirred at 40℃ for 60 min to complete hydrolysis; the hydrolyzate was slowly added to the aerogel suspension at a rate of 1 drop per second, heated to 55℃, and continuously stirred at 250 r / min for 2.5 h; after the reaction was completed, the product was filtered, washed with anhydrous ethanol for 3 times to remove the unreacted coupling agent, and the solid was dried in a vacuum drying oven at 80℃ for 4 h to obtain the surface-grafted modified silica aerogel.
[0036] Preparation Example 2 The preparation method of the phase change energy storage microcapsule is as follows: 50 parts of polyethylene glycol 6000 was heated to 70℃ to melt and keep warm; 20 parts of melamine and 40 parts of formaldehyde were added to 100 parts of deionized water, the pH was adjusted to 8.5, and the mixture was stirred at 60℃ for 90 min for pre-polycondensation to form a transparent pre-polymer aqueous solution; 2 parts of sodium dodecylbenzenesulfonate was added to the pre-polymer aqueous solution as an emulsifier, heated to 75℃, and sheared at a high speed of 3500 r / min for 20 min to disperse the molten polyethylene glycol into small droplets; the pH of the emulsion was adjusted to 4.5, and the mixture was stirred at 65℃ for 3 h to promote the pre-polymer wall material to condense and solidify on the surface of the core material; after the reaction was completed, the mixture was filtered, washed with deionized water until neutral, and dried in a 60℃ air-drying oven for 6 h to obtain phase change energy storage microcapsules with a particle size of 5-20 μm and a tight core-wall combination.
[0037] Preparation Example 3 The preparation method of the amino-modified polyurethane microspheres is as follows: Polyether polyol and toluene diisocyanate were mixed at a molar ratio of 1:2.8, and 150 parts of ethyl acetate were added as a solvent. The mixture was stirred at 70°C for 2 hours to generate an isocyanate-terminated polyurethane prepolymer. 200 parts of deionized water were taken, and 3 parts of polyvinyl alcohol were added as a dispersant and 1 part of gelatin as a stabilizer. After stirring and dissolving, the mixture was heated to 50°C and dispersed into microdroplets by high-speed shearing at 4000 r / min. 50 parts of an aqueous solution containing 8 parts of ethylenediamine were slowly added dropwise to the emulsion, and the mixture was stirred at 45°C for 1.5 hours to carry out a chain extension reaction. Excess ethylenediamine allowed the amino groups to remain on the surface of the microspheres. After the reaction was completed, the mixture was centrifuged at 5000 r / min for 15 minutes, washed four times with deionized water to remove impurities, and dried in a vacuum drying oven at 55°C for 5 hours to obtain amino-modified polyurethane microspheres with a particle size of 1-5 μm and a surface amino content of 0.8-1.5 mmol / g.
[0038] The following are the main raw materials and reagents used in the preparation examples, embodiments, and comparative examples, and their sources and specifications are as follows; unless otherwise specified, all reagents are commercially available analytical grade or higher products: 1. γ-aminopropyltriethoxysilane was purchased from Hubei Zhenbo Chemical Co., Ltd., CAS: 919-30-2; 2. The water-based epoxy resin was purchased from Wuhan Nengren Pharmaceutical Chemical Co., Ltd., with a purity of 99%. 3. The polyamide curing agent was purchased from Shanghai Yuanye Biotechnology Co., Ltd., product number: V30225; 4. Hydroxypropyl methylcellulose was purchased from Shanghai Yuanye Biotechnology Co., Ltd., product number: S14173; 5. Polyethylene glycol 6000 was purchased from Shandong Tiandao Bioengineering Co., Ltd., product number: PEG6000; 6. Melamine-formaldehyde resin was purchased from Wuhan Penglei Biotechnology Co., Ltd., CAS: 9003-08-1; 7. Polyethylene glycol octylphenyl ether was purchased from Shanghai Lianmai Bioengineering Co., Ltd., product number: LM80089C; 8. Sodium dodecyl sulfate was purchased from Shanghai Yuanye Biotechnology Co., Ltd., product number: S15012; 9. The polyether polyol was purchased from Hubei Guangao Biotechnology Co., Ltd., item number: GA0529.
[0039] Example 1 This application provides a high-efficiency and energy-saving building thermal insulation material, which is made of the following components in parts by weight: Modified aerogel 20 parts, composite mineral fiber 25 parts, phase change energy storage microcapsule 11.5 parts, nano silicon dioxide 7.5 parts, water-based epoxy resin 14 parts, polyamide curing agent 5.5 parts, expanded perlite 16 parts, hollow glass microsphere 9 parts, hydroxypropyl methyl cellulose 3.5 parts, amino modified polyurethane microsphere 5 parts, nano boron nitride 4 parts; Among them, the modified aerogel is a silica aerogel surface grafted with a silane coupling agent; the amino modified polyurethane microspheres have a particle size of 3 μm, and the surface amino content is 1.15 mmol / g; Among them, the core material of the phase change energy storage microcapsule is polyethylene glycol 6000, and the wall material is melamine formaldehyde resin; the particle size of the phase change energy storage microcapsule is 12.5 μm; Among them, the sheet thickness of the nano boron nitride is 12.5 nm, and the lateral size is 1.25 μm; the composite mineral fiber includes basalt fiber and ceramic fiber, and the mass ratio of the basalt fiber to the ceramic fiber is 2.5:1.
[0040] The preparation method of the above-mentioned high-efficiency energy-saving building thermal insulation material comprises the following steps: S1, composite mineral fiber pretreatment: after high-temperature activation treatment of the composite mineral fiber, the composite mineral fiber is immersed in a silane coupling agent solution and dried to obtain modified composite mineral fiber; Among them, the temperature of the high-temperature activation treatment is 550℃, and the time is 2.5h; the mass concentration of the silane coupling agent solution is 2%, and the immersion time is 45min; the drying temperature is 110℃, and the time is 1.5h; and the silane coupling agent is γ-aminopropyl triethoxysilane.
[0041] S2, amino modified polyurethane microsphere activation: the amino modified polyurethane microspheres are subjected to plasma treatment to obtain activated polyurethane microspheres; Among them, the plasma treatment is carried out in an argon atmosphere, the treatment frequency is 13.56 MHz, the treatment power is 100 W, the treatment chamber pressure is 15 Pa, and the treatment time is 7.5 min.
[0042] S3, multi-component synergistic dispersion: the phase change energy storage microcapsule, nano boron nitride and the activated polyurethane microspheres obtained in step S2 are dispersed in a liquid medium containing a dispersant by stirring and ultrasonic treatment to obtain a multi-component suspension; Among them, the stirring speed is 4000 r / min, and the time is 25 min; the ultrasonic treatment power is 250 W, and the time is 20 min; after the activated polyurethane microspheres are added, the ultrasonic treatment is continued for 7.5 min; and the dispersant is a compound of polyethylene glycol octyl phenyl ether and sodium dodecyl sulfate in a mass ratio of 2:1, and the addition amount is 1.0% of the total mass of the phase change energy storage microcapsule and the nano boron nitride.
[0043] S4, adhesive system preparation: mix the water-based epoxy resin with the polyamide curing agent, then add the hydroxypropyl methyl cellulose and the nanosilica, continuously stir to form the adhesive system; Wherein, the temperature of mixing is 45℃; the stirring speed when adding the polyamide curing agent is 650r / min, and the mixing time is 12.5min; the stirring time after adding the hydroxypropyl methyl cellulose and the nanosilica is 25min.
[0044] S5, gradient mixture preparation: first, mix the modified composite mineral fiber obtained in step S1 with the expanded perlite, the hollow glass microsphere and the modified aerogel by primary stirring; then, add the multi-component suspension prepared in step S3 for secondary stirring; finally, add the adhesive system prepared in step S4 for tertiary stirring, and mix uniformly under the protection of inert gas; Wherein, the rotation speed of primary stirring is 250r / min, and the time is 12.5min; the rotation speed of secondary stirring is 900r / min, and the time is 25min; the rotation speed of tertiary stirring is 1750r / min, and the time is 35min; the inert gas is nitrogen, and the gas inlet rate is 0.75L / min.
[0045] S6, molding and post-processing: inject the mixed material obtained in step S5 into a preheated mold for compression molding and demolding; heat treat the demolded molding blank; finally, cure under the condition of controlled temperature and humidity to obtain the building thermal insulation material; Wherein, the preheating temperature of the mold is 70℃, the compression pressure is 6.5MPa, and the pressure holding time is 17.5min; the heat treatment is carried out at 175℃ for 2.5h, the heating rate is 7.5℃ / min, and the heat treated product is naturally cooled to room temperature; the curing environment temperature is 27.5℃, the relative humidity is 65%, and the curing time is 9 days.
[0046] Example 2 The embodiment of the present application provides a kind of high efficiency energy-saving building thermal insulation material, which is made of the following components by weight: Modified aerogel 15 parts, composite mineral fiber 20 parts, phase change energy storage microcapsule 8 parts, nanosilica 5 parts, water-based epoxy resin 10 parts, polyamide curing agent 3 parts, expanded perlite 12 parts, hollow glass microsphere 6 parts, hydroxypropyl methyl cellulose 2 parts, amino modified polyurethane microsphere 3 parts, nanometer boron nitride 2 parts; Wherein, the modified aerogel is a silica aerogel grafted with a silane coupling agent on the surface; the amino modified polyurethane microsphere has a particle size of 1 μm, and the surface amino content is 0.8 mmol / g; Wherein, the core material of the phase change energy storage microcapsule is polyethylene glycol 6000, the wall material is melamine formaldehyde resin, and the particle size of the phase change energy storage microcapsule is 5 μm. The nanometer boron nitride has a sheet thickness of 5 nm and a lateral size of 0.5 μm; and the composite mineral fiber comprises basalt fiber and ceramic fiber, and the mass ratio of the basalt fiber to the ceramic fiber is 2:1.
[0047] The preparation method of the high-efficiency and energy-saving building thermal insulation material comprises the following steps: S1, composite mineral fiber pretreatment: after high-temperature activation treatment of the composite mineral fiber, the composite mineral fiber is immersed in a silane coupling agent solution and dried to obtain modified composite mineral fiber; The temperature of the high-temperature activation treatment is 500 DEG C, and the time is 2 h; the mass concentration of the silane coupling agent solution is 1%, and the immersion time is 30 min; the drying temperature is 100 DEG C, and the time is 1 h; and the silane coupling agent is gamma-aminopropyl triethoxysilane.
[0048] S2, amino-modified polyurethane microsphere activation: the amino-modified polyurethane microspheres are subjected to plasma treatment to obtain activated polyurethane microspheres; The plasma treatment is carried out in an argon atmosphere, the treatment frequency is 13.56 MHz, the treatment power is 80 W, the treatment chamber pressure is 10 Pa, and the treatment time is 5 min.
[0049] S3, multi-component synergistic dispersion: the phase change energy storage microcapsules, the nanometer boron nitride and the activated polyurethane microspheres obtained in step S2 are dispersed in a liquid medium containing a dispersant by stirring and ultrasonic treatment to obtain a multi-component suspension; The stirring speed is 3000 r / min, and the time is 20 min; the ultrasonic treatment power is 200 W, and the time is 15 min; the activated polyurethane microspheres are continuously treated by ultrasonic treatment for 5 min after being added; and the dispersant is a compound of polyethylene glycol octylphenyl ether and sodium dodecyl sulfate in a mass ratio of 2:1, and the addition amount is 0.5% of the total mass of the phase change energy storage microcapsules and the nanometer boron nitride.
[0050] S4, preparation of a bonding system: the water-based epoxy resin and the polyamide curing agent are mixed, and then the hydroxypropyl methyl cellulose and the nanometer silicon dioxide are added, and continuous stirring is performed to form a bonding system; The mixing temperature is 40 DEG C; the stirring speed is 500 r / min when the polyamide curing agent is added, and the mixing time is 10 min; and the stirring time after the hydroxypropyl methyl cellulose and the nanometer silicon dioxide are added is 20 min.
[0051] S5, gradient mixture material preparation: first, the modified composite mineral fiber obtained in step S1 is mixed with expanded perlite, hollow glass microspheres and modified aerogel by primary stirring; then, the multi-component suspension prepared in step S3 is added for secondary stirring; finally, the bonding system prepared in step S4 is added for tertiary stirring, and the mixture is uniformly mixed under the protection of inert gas; wherein the rotation speed of the primary stirring is 200 r / min, and the time is 10 min; the rotation speed of the secondary stirring is 800 r / min, and the time is 20 min; the rotation speed of the tertiary stirring is 1500 r / min, and the time is 30 min; the inert gas is argon, and the gas inlet rate is 0.5 L / min.
[0052] S6, molding and post-processing: the mixture obtained in step S5 is injected into a preheated mold for compression molding and demolding; the molded body after demolding is subjected to heat treatment; finally, curing is carried out under controlled temperature and humidity conditions to obtain a building thermal insulation material; wherein the preheating temperature of the mold is 60℃, the compression pressure is 5 MPa, and the pressure holding time is 15 min; the heat treatment is carried out at 150℃ for 2 h, and the heating rate is 5℃ / min, and the heat treatment is naturally cooled to room temperature after heat treatment; the curing environment temperature is 25℃, the relative humidity is 60%, and the curing time is 7 days.
[0053] Example 3 The embodiment of the present application provides a kind of high efficiency energy-saving building thermal insulation material, which is made of the following components by weight: Modified aerogel 25 parts, composite mineral fiber 30 parts, phase change energy storage microcapsule 15 parts, nano silicon dioxide 10 parts, water-based epoxy resin 18 parts, polyamide curing agent 8 parts, expanded perlite 20 parts, hollow glass microspheres 12 parts, hydroxypropyl methyl cellulose 5 parts, amino modified polyurethane microspheres 7 parts, nano boron nitride 6 parts; Wherein, the modified aerogel is a silica aerogel surface grafted with silane coupling agent; the particle size of the amino modified polyurethane microspheres is 5 μm, and the surface amino content is 1.5 mmol / g; Wherein, the core material of the phase change energy storage microcapsule is polyethylene glycol 6000, and the wall material is melamine formaldehyde resin; the particle size of the phase change energy storage microcapsule is 20 μm. Wherein, the sheet thickness of the nano boron nitride is 20 nm, and the lateral size is 2 μm; the composite mineral fiber includes basalt fiber and ceramic fiber, and the mass ratio of basalt fiber to ceramic fiber is 3:1.
[0054] The above method for preparing a high-efficiency energy-saving building thermal insulation material includes the following steps: S1, composite mineral fiber pretreatment: after high temperature activation treatment of the composite mineral fiber, then impregnated and dried in silane coupling agent solution, the modified composite mineral fiber is obtained; Among them, the temperature of high temperature activation treatment is 600℃, the time is 3h; the mass concentration of silane coupling agent solution is 3%, the impregnation time is 60min; the drying temperature is 120℃, the time is 2h; and the silane coupling agent is γ-aminopropyl triethoxysilane.
[0055] S2, amino modified polyurethane microspheres activation: the amino modified polyurethane microspheres are treated by plasma to obtain activated polyurethane microspheres; Among them, the plasma treatment is carried out in argon atmosphere, the treatment frequency is 13.56MHz, the treatment power is 120W, the treatment chamber pressure is 20Pa, and the treatment time is 10min.
[0056] S3, multi-component synergistic dispersion: the phase change energy storage microcapsule, nano boron nitride and the activated polyurethane microspheres obtained in step S2 are dispersed in a liquid medium containing a dispersant by stirring and ultrasonic treatment to obtain a multi-component suspension; Among them, the stirring speed is 5000r / min, the time is 30min; the ultrasonic treatment power is 300W, the time is 25min; after adding the activated polyurethane microspheres, continue to ultrasonic treatment for 10min; and the dispersant is polyethylene glycol octyl phenyl ether and sodium dodecyl sulfate compounded according to the mass ratio of 2:1, and the addition amount is 1.5% of the total mass of the phase change energy storage microcapsule and nano boron nitride.
[0057] S4, preparation of bonding system: mixing water-based epoxy resin and polyamide curing agent, then adding hydroxypropyl methyl cellulose and nano silicon dioxide, and continuously stirring to form the bonding system; Among them, the mixing temperature is 50℃; the stirring speed is 800r / min when the polyamide curing agent is added, and the mixing time is 15min; the stirring time after adding hydroxypropyl methyl cellulose and nano silicon dioxide is 30min.
[0058] S5, gradient mixture preparation: first, the modified composite mineral fiber obtained in step S1 is mixed with expanded perlite, hollow glass microspheres and modified aerogel by primary stirring; then the multi-component suspension prepared in step S3 is added for secondary stirring; finally, the bonding system prepared in step S4 is added for tertiary stirring, and the mixture is uniformly mixed under the protection of inert gas; Among them, the primary stirring speed is 300r / min, the time is 15min; the secondary stirring speed is 1000r / min, the time is 30min; the tertiary stirring speed is 2000r / min, the time is 40min; the inert gas is nitrogen, and the gas inlet rate is 1L / min.
[0059] S6, molding and post-processing: injecting the mixture obtained in step S5 into a preheated mold for compression molding and demolding; performing heat treatment on the demolded molded body; and finally performing curing under a controlled temperature and humidity condition to obtain the building thermal insulation material; The preheating temperature of the mold is 80℃, the compression pressure is 8MPa, and the pressure holding time is 20min; the heat treatment is performed at 200℃ for 3h, the heating rate is 10℃ / min, and the heat treatment is naturally cooled to room temperature after the heat treatment; the curing environment temperature is 30℃, the relative humidity is 70%, and the curing time is 10 days.
[0060] Comparative Example 1 The only difference between this comparative example and Example 1 is that the amino-modified polyurethane microspheres are deleted from the components, and the types, weight parts, and preparation methods of the remaining components are completely consistent with Example 1.
[0061] Comparative Example 2 The only difference between this comparative example and Example 1 is that the silica aerogel modified by surface grafting with a silane coupling agent is replaced by unmodified ordinary silica aerogel, and the types, weight parts, and preparation methods of the remaining components are completely consistent with Example 1.
[0062] Comparative Example 3 The only difference between this comparative example and Example 1 is that the nano boron nitride is deleted from the components, and the types, weight parts, and preparation methods of the remaining components are completely consistent with Example 1.
[0063] Comparative Example 4 The only difference between this comparative example and Example 1 is that the amino-modified polyurethane microspheres are not subjected to plasma treatment in step S2, and the unactivated amino-modified polyurethane microspheres are directly used in step S3, and the types, weight parts, and preparation methods of the remaining steps are completely consistent with Example 1.
[0064] Comparative Example 5 This comparative example is a conventional polyurethane hard foam thermal insulation material, which uses a commercially available conventional polyurethane hard foam thermal insulation material. The main components are polyurethane prepolymer, blowing agent, and flame retardant, without modified aerogel, amino-modified polyurethane microspheres, and nano boron nitride. The preparation process is conventional foaming and curing molding, without plasma activation, gradient mixing, and heat treatment steps.
[0065] Comparative Example 6 This comparative example is a conventional rock wool insulation board, which uses a commercially available conventional rock wool insulation board. The main components are basalt fibers and phenolic resin binder, without phase change energy storage microcapsules, nano silica, and hollow glass microspheres. The preparation process is melt spinning, molding, and curing, without multi-component synergistic dispersion and gradient mixing steps.
[0066] I. Thermal conductivity test The test was conducted in accordance with GB / T10294-2008 "Determination of Steady-State Thermal Resistance and Related Properties of Thermal Insulation Materials - Protective Hot Plate Method".
[0067] The building insulation materials prepared in Examples 1-3 and Comparative Examples 1-6 were selected, and each sample was processed into a standard specimen of 300mm×300mm×50mm. Three parallel specimens were prepared for each sample. Before testing, all specimens were pretreated in an environment of 23℃ and 50% relative humidity for 24 hours to ensure that the moisture content of the specimens was in equilibrium with the environment. Using a protective hot plate thermal conductivity meter, with the cold plate temperature set to 10℃ and the hot plate temperature to 30℃, the heat flux and temperature difference of each specimen were measured under steady-state conditions, and the thermal conductivity was calculated as the average value of the three parallel specimens. This test directly reflects the thermal insulation capacity of the material. The lower the value, the better the energy-saving effect. It can compare the thermal conductivity differences between the examples and comparative examples, especially the existing polyurethane rigid foam rock wool, highlighting the synergistic thermal insulation effect of modified aerogel and nano boron nitride.
[0068] II. Compressive Strength Test The test was conducted in accordance with GB / T1041-2008 "Determination of compressive properties of plastics".
[0069] The materials from Examples 1-3 and Comparative Examples 1-6 were processed into standard cubic specimens of 50mm × 50mm × 50mm, with five parallel specimens prepared for each sample. Before testing, all specimens were pretreated for 24 hours at 23℃ and 50% relative humidity. A universal testing machine was used for compression testing, with a loading speed of 2mm / min. Loading continued until the specimen showed significant damage or deformation reached 10% of its height. The maximum pressure value at specimen failure was recorded. The compressive strength was calculated based on the pressure and the stress area of the specimen, and the average value of the five parallel specimens was taken, with outliers discarded.
[0070] III. Thermal Aging Insulation and Strength Retention Rate Test The test was conducted in accordance with the heat aging test method in GB / T14683-2017 "Silicone and Modified Silicone Building Sealants" and the aforementioned two test standards.
[0071] Select the standard test piece of each example and comparative example, prepare 300 mm x 300 mm x 50 mm size test piece for thermal conductivity test, prepare 50 mm x 50 mm x 50 mm size test piece for compressive strength test, each size 3; all test pieces are placed in a heat aging test chamber, set the aging temperature to 80℃, continue aging for 1000 hours, keep the air circulating in the test chamber during the aging process; after aging, all test pieces are taken out and placed in an environment with a temperature of 23℃ and a relative humidity of 50% for cooling for 24 hours; after cooling, the thermal conductivity and compressive strength of the two types of test pieces after aging are determined again according to the same method as the thermal conductivity test and compressive strength test before. Calculate the thermal conductivity retention rate and compressive strength retention rate of each sample after heat aging, the higher the retention rate, the better the long-term stability of the material; wherein, thermal conductivity retention rate = thermal conductivity after aging / thermal conductivity before aging x 100%; compressive strength retention rate = compressive strength after aging / compressive strength before aging x 100%.
[0072] The performance test data of the building thermal insulation material are shown in Table 1.
[0073] Table 1:
[0074] It can be seen from Examples 1-3 and Comparative Example 1 that the amino-modified polyurethane microspheres play an important role in the building thermal insulation material, and their presence or absence will affect the structural integrity and long-term stability of the material. The microspheres can form a good interfacial bond with other components through their own properties, which not only helps to improve the load-bearing capacity of the material, but also plays a certain self-repairing or structural reinforcing role during the heat aging process. Without this component, the overall performance synergy of the material is weakened, and the long-term retention effect of the related performance is obviously affected.
[0075] It can be seen from Examples 1-3 and Comparative Example 2 that the surface grafting modification treatment of silica aerogel by silane coupling agent is not a redundant step, and the modified aerogel can better integrate into the material system. The modification treatment probably improves the compatibility of the aerogel with other components, reduces the interfacial defects, makes it more difficult for heat transfer paths to form, and also enhances the bonding strength of the aerogel and the matrix. The ordinary silica aerogel without modification has deficiencies in compatibility and bonding strength, and cannot fully play the synergistic role of thermal insulation and structural support.
[0076] It can be seen from Examples 1-3 and Comparative Example 3 that nanometer boron nitride is a key synergistic component in the thermal insulation system of the material, which can form an efficient heat insulation network in combination with components such as modified aerogel. The lamellar structure of nanometer boron nitride may have a physical barrier effect on heat transfer, which cooperates with the low thermal conductivity of modified aerogel to further optimize the heat insulation effect. Meanwhile, its structural characteristics can also help to improve the structural stability of the material to a certain extent. Without this component, the synergistic effect of the heat insulation system is broken, and the thermal insulation performance and long-term stability of the material are affected.
[0077] It can be seen from Examples 1-3 and Comparative Example 4 that the plasma activation treatment of the amino-modified polyurethane microspheres is an important process to ensure the performance of the material. Plasma treatment can improve the surface activity of the microspheres, making them more easily interact with other components to form a stronger bonding interface, thereby better playing the role of reinforcement and long-term stability. The surface activity of the microspheres without activation treatment is insufficient, and the bonding force with other components is weak, making it difficult to fully integrate into the material system, resulting in a decline in the related performance and long-term retention effect of the material.
[0078] It can be seen from Examples 1-3 and Comparative Example 5 that the modified aerogel, amino-modified polyurethane microspheres, nanometer boron nitride, and other core components in the present application, as well as the specific processes such as plasma activation, gradient mixing, and heat treatment, collectively form the basis for the excellent performance of the material. The existing polyurethane hard foam thermal insulation material lacks these core components and key processes, and cannot form a multi-component synergistic system. Heat transfer is difficult to effectively block, and the load-bearing capacity and anti-aging ability of the material structure are relatively weak. The overall performance of the product is significantly different from the product of the present application.
[0079] It can be seen from Examples 1-3 and Comparative Example 6 that the multi-component matching design and fine preparation process used in the present application are the key to improving the comprehensive performance of the material. The existing rock wool insulation board has relatively single components, lacks functional components such as phase change energy storage microcapsules and nanometer silicon dioxide, and does not use multi-component synergistic dispersion and gradient mixing processes. This results in the material being unable to form an efficient heat insulation network in terms of heat insulation performance, and the structural bonding strength and anti-aging performance are also limited due to the lack of synergistic effect between components, making it difficult to achieve the comprehensive performance level of the product of the present application.
[0080] This specific embodiment is merely an explanation of the present application and is not a limitation thereof. Those skilled in the art can make modifications to this embodiment without creative contribution after reading the present specification, but as long as it is within the scope of the claims of the present application, it is protected by the patent law.
Claims
1. A high-efficiency and energy-saving building thermal insulation material, characterized in that: It is made of the following components by weight: modified aerogel 15-25 parts, composite mineral fiber 20-30 parts, phase change energy storage microcapsule 8-15 parts, nano silicon dioxide 5-10 parts, water-based epoxy resin 10-18 parts, polyamide curing agent 3-8 parts, expanded perlite 12-20 parts, hollow glass microbeads 6-12 parts, hydroxypropyl methyl cellulose 2-5 parts, amino modified polyurethane microspheres 3-7 parts, and nano boron nitride 2-6 parts.
2. The energy efficient building thermal insulation material according to claim 1, characterized in that: The modified aerogel is a silica aerogel surface grafted with a silane coupling agent; the amino modified polyurethane microspheres have a particle size of 1-5 μm, and the surface amino content is 0.8-1.5 mmol / g.
3. The energy efficient building thermal insulation material according to claim 1, characterized in that: The core material of the phase change energy storage microcapsule is polyethylene glycol 6000, and the wall material is melamine formaldehyde resin; the phase change energy storage microcapsule has a particle size of 5-20 μm; and the nano boron nitride has a sheet thickness of 5-20 nm and a lateral size of 0.5-2 μm.
4. The energy efficient building thermal insulation material according to claim 1, characterized in that: The composite mineral fiber includes basalt fiber and ceramic fiber, and the mass ratio of basalt fiber to ceramic fiber is 3:1-2:
1.
5. A method for preparing a high-efficiency energy-saving building thermal insulation material, characterized in that, A high-efficiency energy-saving building thermal insulation material according to any one of claims 1-4, comprising the following steps: S1, composite mineral fiber pretreatment: the composite mineral fiber is subjected to high-temperature activation treatment, then immersed in a silane coupling agent solution and dried to obtain modified composite mineral fiber; S2, amino modified polyurethane microsphere activation: the amino modified polyurethane microspheres are subjected to plasma treatment to obtain activated polyurethane microspheres; S3, multi-component synergistic dispersion: the phase change energy storage microcapsule, nano boron nitride and activated polyurethane microspheres obtained in step S2 are dispersed in a liquid medium containing a dispersant by stirring and ultrasonic treatment to obtain a multi-component suspension; S4, adhesive system preparation: the water-based epoxy resin and polyamide curing agent are mixed, then hydroxypropyl methyl cellulose and nano silicon dioxide are added, and continuous stirring is performed to form an adhesive system; S5, gradient mixture preparation: the modified composite mineral fiber obtained in step S1 is first mixed with expanded perlite, hollow glass microbeads and modified aerogel by primary stirring; then the multi-component suspension prepared in step S3 is added for secondary stirring; finally, the adhesive system prepared in step S4 is added for tertiary stirring, and the mixture is uniformly mixed under inert gas protection; S6, molding and post-processing: the mixture obtained in step S5 is injected into a preheated mold for compression molding and demolding; the molded body after demolding is subjected to heat treatment; and finally, curing is performed under controlled temperature and humidity conditions to obtain the building thermal insulation material.
6. The method according to claim 5, wherein the method is characterized by: In step S1, the temperature of the high-temperature activation treatment is 500-600℃, and the time is 2-3h; the mass concentration of the silane coupling agent solution is 1-3%, and the immersion time is 30-60min; the drying temperature is 100-120℃, and the time is 1-2h; and the silane coupling agent is γ-aminopropyl triethoxysilane; in step S2, the plasma treatment is carried out in an argon atmosphere, the treatment frequency is 13.56MHz, the treatment power is 80-120W, the treatment chamber pressure is 10-20Pa, and the treatment time is 5-10min.
7. The method according to claim 5, wherein the method is characterized by: In step S3, the stirring speed is 3000-5000r / min, and the time is 20-30min; the ultrasonic treatment power is 200-300W, and the time is 15-25min; after the activated polyurethane microspheres are added, the ultrasonic treatment is continued for 5-10min; and the dispersing agent is a compound of polyethylene glycol octylphenyl ether and sodium dodecyl sulfate in a mass ratio of 2:1, and the addition amount is 0.5-1.5% of the total mass of the phase change energy storage microcapsules and the boron nitride nanoparticles.
8. The method according to claim 5, wherein the method is characterized by: In step S4, the mixing temperature is 40-50℃; when the polyamide curing agent is added, the stirring speed is 500-800r / min, and the mixing time is 10-15min; and after the hydroxypropyl methyl cellulose and the nanosilica are added, the stirring time is 20-30min.
9. The method according to claim 5, wherein the method is characterized by: In step S5, the first-stage stirring speed is 200-300r / min, and the time is 10-15min; the second-stage stirring speed is 800-1000r / min, and the time is 20-30min; the third-stage stirring speed is 1500-2000r / min, and the time is 30-40min; the inert gas is nitrogen or argon, and the gas inlet rate is 0.5-1L / min.
10. The method for preparing a high-efficiency energy-saving building thermal insulation material according to claim 5, characterized in that: In step S6, the mold preheating temperature is 60-80℃, the pressing pressure is 5-8MPa, and the pressure maintaining time is 15-20min; the heat treatment is carried out at 150-200℃ for 2-3h, the heating rate is 5-10℃ / min, and after the heat treatment, the natural cooling is carried out to room temperature; the curing environment temperature is 25-30℃, the relative humidity is 60-70%, and the curing time is 7-10 days.
Citation Information
Patent Citations
Efficient energy-saving building heat preservation material and preparation method thereof
CN108675685A
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